The structure and ion conductivity of Nd2Mo2O9powders were synthesized by using Nd(NO2)3, MoO3, and aspartic acid (fuel) in assisted combustion method with heating at 550˚C for 6 hours. The thermal decomposition, phase identification, morphology, ionic conductivity of the samples were studied by TGA/DTA, XRD and SEM four probe D.C. method respectively. The formation of Nd2Mo2O9 was confirmed by FTIR studies. The synthesis and crystallization were followed by thermochemical techniques (TGA/DTA) studies. The synthesized materials showed reasonable ionic conductivity. These results indicate that assisted combustion method is a promising method to prepare nanocrystalline Nd2Mo2O9 for solid oxide fuel cell.

1. Rajasekhar .M, Kalaivani, N; International Journal of Advance Research, Ideas and Innovations in Technology.
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ISSN: 2454-132X
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(Volume3, Issue1)
Preparation, Structure, and Characterization of Nd2mo2o9 fast
Oxide Ion Conductor
M. Rajasekhar
Advanced Energy Research Lab,
PG& Research Department of chemistry,
Government Arts College, Dharmapuri-636 705, South India.
Energylag20@gmail.com
N. Kalaivani
Advanced Energy Research Lab,
PG& Research Department of chemistry,
Government Arts College, Dharmapuri-636 705, South India.
Energylag20@gmail.com
Abstract: The structure and ion conductivity of Nd2Mo2O9powders were synthesized by using Nd(NO2)3, MoO3, and aspartic acid
(fuel) in assisted combustion method with heating at 550˚C for 6 hours. The thermal decomposition, phase identification,
morphology, ionic conductivity of the samples were studied by TGA/DTA, XRD and SEM four probe D.C. method respectively.
The formation of Nd2Mo2O9 was confirmed by FTIR studies. The synthesis and crystallization were followed by thermochemical
techniques (TGA/DTA) studies. The synthesized materials showed reasonable ionic conductivity. These results indicate that
assisted combustion method is a promising method to prepare nanocrystalline Nd2Mo2O9 for solid oxide fuel cell.
Keywords: Ionic Conductivity, Scanning Electron Microscopy, Transmission Electron Microscope, X-ray Diffraction, and FTIR.
I. INTRODUCTION
Solid oxide fuel cells (SOFCs) which convert chemical energy directly into electrical energy have been viewed as promising new
power-generating systems and true multi-fuel energy devices. Recently significant efforts have been directed towards the
development of intermediate temperature solid oxide fuel cell (IT-SOFC) due to its high power density and high working efficiency
when operated around 500-800˚C. Mixed ionic-electronic conductivity (MIECs) have attracted the attention of researchers due to
high thermal and chemical stability along with high oxygen diffusion and electronic conductivity.
The efficiency of energy conversion of an SOFC and its performance durability mainly depend on the oxide ion conducting
solid electrolyte activity. The Neodymium molybdate forms a large family of materials with interesting physical properties. These
properties depend on the crystal structures of these oxides, as well as on the oxidation state of molybdenum. In the case of the
highest oxidation state of molybdenum +VI, the recent discovery of the fast oxide-ion conductor, La2Mo2O9 has attracted
considerable interest for its potential applications.
In the present work, synthesis of Nd2Mo2O9nano powders using different molar ratios by assisted combustion method. The
effect of different ratios on phase evaluation, size, and shape of the Nd2Mo2O9particles were studied. Oxide materials with high
mobility of oxygen ion receive extensive attention owing to the potential applications in solid oxide fuel cells, oxygen sensors,
oxygen pumps, and oxygen-permeable membrane catalysts.
II.EXPERIMENTAL AND CHARACTERIZATION
ThenanocrystallineNd2Mo2O9powder was synthesized by assisted combustion method using high purity Nd(NO3)2(Sigma Aldrich,
>99.9%), MoO3(Sigma-Aldrich, >99.9%), and aspartic acid (Sigma Aldrich, >99.9%), as fuel. All of the reagents, in requisite
stoichiometry amounts of the starting materials, were dissolved in the double distilled deionized water in order to obtain a
homogeneous solution. A gel was appeared after continuous stirring at 80˚C for depending on the element. The foamy powder was
crushed in a pestle and mortar. The crushed powder was kept in a muffle furnace at 600°C for hours 6 to get a single- phase
nanocrystalline powders.
III. STRUCTURAL CHARACTERIZATION ANALYSIS
The structural properties of the synthesized material using X-ray diffraction studies (Model: Philips X pert MPD). The diffraction
patterns were recorder using Cu-Kα radiation at room temperature in the range of 10˚≤ 2θ≤70˚. The X-ray data were recorded in
terms of the diffracted X-ray intensities (I) vs 2θ. The crystalline size was calculated with the help of scherrer’
s formula, which is
given as
D =0.9λ/βcosθ,

2. Rajasekhar .M, Kalaivani, N; International Journal of Advance Research, Ideas and Innovations in Technology.
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Where D is the crystallite size, β is the full-width at half-maximum (FWHM) of the most intensity W diffraction peak in radians, θ
is the diffraction angle and λ is the wave length of X-ray radiation. The particle size and morphology of the produced powder were
analysed with a JEOL scanning electron microscopy SEM (Model: JSM-840A) equipment.
The thermal decomposition of the polymeric precursors was characterized by perkin-Elmer TG/DTA thermal analysis
(Model; Pyris Diamond). The TGA is a process which relies on measuring the change in physical and chemical properties of a
sample as a function of temperature or as a function of time.
IV.Result and Discussion
a. Analysis of Crystal Structure
Typical X-ray powder diffraction (XRD) patterns of Nd2Mo2O9is shown in Fig 4.1. In general, all the diffracted peaks are broader
than usually observed for highly crystalline powder. The lattice parameter calculated for the synthesizedNd2Mo2O9, the broadening
of the diffracted peaks is attributed to the superfine crystalline nature of composites. These results are in good agreement with the
result of the orthorhombic structure. The size of the particles was calculated by Scherrer equation it was 30 nm. All diffraction peaks
of the samples can be indicated to the orthorhombic structure without the formation of other impurities. The particles of the
synthesized products are in nano range.
Fig. 1.X-ray diffraction pattern of Nd2Mo2O9
b. Scanning Electron Microscopy
Fig.4.2 shows the SEM microstructure of Nd2Mo2O9 powder obtained at 550°C for 6 hours. The surface morphology of the
synthesized product was different pores and grains. Further, the SEM image indicates that the particles are agglomeration. The
average crystallite size was 30 nm. The particles are uniformly distributed. There is an agglomerate of the particles. The particles
of the synthesized products are in nano range
Fig.2.SEM photograph of Nd2Mo2O9
c. Thermal Analysis
TGA/DTA
Fig 4.3.shows that TGA/DTA pattern obtained on Nd2Mo2O9 powder. In the TGA pattern, the Nd2Mo2O9 sample showed a weight
loss of about 0.052 mg/min until 100˚C. The sample on further heating from 100˚C-800˚C showed slight weight gain and loss of
about 0.052mg/min. Again the sample showed a weight increase from 109.43˚C-386.39˚C of 0.688mg/min. The weight gain and
weight loss indicated that the Nd2Mo2O9 powder exhibited easily reversible absorption-desorption of oxygen from the air. The
chemical decomposition with increases of temperature was examined through DTA and it appeared as the endothermic and
exothermic peaks in the DTA curve. From the DTA curve, it is seen that a broad exothermic peak at 586.830˚C occurred due to

3. Rajasekhar .M, Kalaivani, N; International Journal of Advance Research, Ideas and Innovations in Technology.
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weight lose between 39.92˚C-723.50˚C in TGA curve. From the above TGA/DTA data, we know the Nd2Mo2O9gradually absorbs
the oxygen from air with temperature.
Fig. 3.TGA and DTA of Nd2Mo2O9
d. FTIR Analysis
FTIR spectroscopy was used to verify the functional groups present in the crystalline substance which range of 4000 cm-1
to400cm-
1
as shown in fig.4.4. The broadband at 3600.9cm-1
can be assigned to vibration mode of chemically bonded hydroxyl groups. The
powder exhibited a strong bond at 600-1000 cm-1
due to the stretching mode of Mo-O bond in the structure. The peak appeared at
816.1 cm-1
corresponds to the H-O-H bond mode confirming the presence of moisture in the sample. The peak appeared at 1354.6
cm -1
is due to the presence of CO2 in the sample. The sampleNd2Mo2O9 exhibited a low-intensity peak at 816.1 cm -1
sample
exhibited two peaks obtained between the wavelength regions 800-1400 cm-1
and observed at 816.1, 1354.6, and 3600.9 cm -1
. The
peak appeared at 1354.6 cm-1
is related to the O-H stretching vibration of H2O in the sample. The broadband at 3600.9cm-1
can be
assigned to vibration mode of chemically bonded hydroxyl groups.
Fig 4.FT-IR spectrum of Nd2Mo2O9
e. Ionic Conductivity and its Temperature Dependence
The ionic conductivity of Nd2Mo2O9 at 800˚C is used for SOFC electrolyte application. The Arrhenius plot for the overall
conductivity of Nd2Mo2O9 pellet sintered at 800˚C for 6 h is shown in 4.5. It shows clearly a first-order transition at 560˚C with the
increasing conductivity. At 750˚C it exhibits a conductivity of 0.160S/cm. The estimated ionic transport number is slightly decreased
with increasing temperature. This result demonstrates that the conductivity of Nd2Mo2O9 is mainly ionic in nature.

4. Rajasekhar .M, Kalaivani, N; International Journal of Advance Research, Ideas and Innovations in Technology.
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Fig. 5. Arrhenius plot of the overall conductivity of Nd2Mo2O9 pellet sintered at 800˚C for 6 h
CONCLUSION
The present investigation was carried out to improve the performance of Nd2Mo2O9 by the synthesis method. The electrochemical
behavior of Nd2Mo2O9 based materials depends upon the method of synthesis and sintering temperature nanocrystalline materials.
The present work was mainly focused on synthesis and ionic conductivity of Nd2Mo2O9.
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